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polar solvents. The positive end of water can be attracted to the negative ions in ionic
networks. Likewise, the negative end of water can be attracted to the positive ions.
One by one, the ions in ionic network solids can be "plucked" away and surrounded
by polar solvent molecules and dispersed randomly throughout the solution. Do you
think that ionic network solids are soluble in non-polar solvents?
Molecular network solids are more difficult to distinguish by solubility because the
individual molecules in these networks can either be polar or non-polar. As a general
rule, "like dissolves like" meaning that non-polar molecules dissolve in non-polar
solvents and vice versa.
Experimental Procedures:
<Take notes on a brief video depicting an ionic network solid being dissolved by
water molecules>
Your lab instructor will have a series of labeled beakers containing a variety of
common solvents. Your instructor will attempt to dissolve sodium chloride, graphite,
and sugar in each of these solvents. Record detailed observations of the results, and
write an explanation for each observation given your knowledge of solubility and
solids. You probably don't know whether sugar (sucrose) is a polar or non-polar
molecular network solid. Make sure you describe how you can tell from the solubility
results.
Table 1. Solvents used in solubility tests
Solvent
Description
Water
polar
Methanol
polar
Acetone
polar
Hexane
non-polar
Toluene
non-polar
Benzene
non-polar
For the rest of the lab you will prepare solutions for crystal growth. In groups of three
students, clean and dry three 250 mL beakers. These should be rinsed with distilled
water prior to drying. Prepare and label the following solutions:
Beaker# 1. 40g NaNO3 + 50 mL distilled water
2. 20g K3Fe(CN)6 + 50 mL distilled water
3. 20g KAl(SO4)2.12H2O + 100 mL distilled water
Place each beaker on a hot plate located in the hoods at each bench. Add a stir bar to
each beaker and stir the solution continually while heating it using a medium setting.
Don't allow too much water to evaporate as this will reduce the amount of solid that
will dissolve. When all the solid has gone into solution, remove the beakers from the
hot plates and set them aside to cool.
After the solutions have cooled to room temperature, if no crystals have begun to
form, drop about 6 flecks of additional solid in the solution. These will serve as
crystallization sites. Cover the beakers with a watch glass making sure there remains a
small opening at the beaker spout which will allow the water to evaporate slowly. Set
the beakers in your lab drawer so they may sit undisturbed until the following week.
Questions
1) Your conclusions from the solubility tests were dependent on having some previous
knowledge of the properties of the solute and solvent. How well do you think
solubility would work for determining a completely unknown solute? Which kinds of
crystalline solids are the easiest to determine with solubility tests? Which are
ambiguous?
2) You know that NaNO3, K3Fe(CN)6, and KAl(SO4)2 all dissolve in water. With
what you know about solubility, can you classify these pure crystalline solids into the
categories in Figure 1? Can any categories be rules out?
SESSION #2
Objectives:
*Prepare seed crystals for alum and potassium ferricyanide.
*Build models to demonstrate glide planes.
Growing larger crystals
The starting materials you used in the first session were the solids in a powdery form.
These powders are still crystals, but only very tiny ones. In order for single crystals to
grow in an extended orderly fashion they must be allowed to grow slowly so that each
new atom can migrate to its favored position. Last session you started growing
crystals with saturated solutions of the various solids. The term saturated means that
the maximum amount of solute was dissolved in the solvent. Over the week, the
solvent evaporated, leaving the solution supersaturated. That is, there was not enough
solvent left for the solute to remain dissolved. Instead, the solute reordered itself and
formed a solid known as a precipitate. If this reordering process is too fast, you will
just get the powder back out of the water. Instead, you probably formed several small
crystals on the bottom of your beaker. The goal of this session will be to start growing
one large single crystal of each solid.
When crystals of alum and potassium ferricyanide form on the bottom or sides of
containers , they are sometimes distorted because the growth of the crystal is
restricted. A solution to this problem is to grow your crystal away from the surface of
the container in the center of the solution. You will suspend a seed crystal by a thread
in the center of your solution to allow unrestricted growth to occur. The crystals of
NaNO3 grow with a flat edge all along the beaker surface, so you will not need to
suspend these crystals.
Seed crystals are just normal crystals which trigger further crystal growth on top of
themselves. Disordered ions are more likely to reorder themselves on a seed crystal
(which already has an extending ordered structure) than they are to start a new crystal
on their own. As you might imagine, the success of your large single crystal depends
greatly on having a high quality seed crystal as a foundation. Each of the solids you
will be growing crystals from will have a different shape according to their
arrangement of the atoms and how fast each face of the crystal grows.
Glide Planes
Crystalline substances often consistently break along specific planes in the crystal.
You will be using two different kinds of modeling kits to explore the origins of glide
planes in crystalline substances. Consider the representation of graphite in Figure 2
below. The vertices of the hexagons represent the carbon atoms, and imaginary planes
have been superimposed to enhance the visibility of the graphite layers. In reality,
these sheets would extend for miles to represent just a pencil point of graphite. A
corner of the sheet is enlarged so you can better see the local structure of graphite.
The dotted lines in the blown-up representation are meant as a visual aid; they show
which atoms line up between layers.
covalent bonds and "atomic stickiness" (by the way, chemists actually call this "van
der Waals forces") has important consequences. First, it explains why there is a
greater distance between sheets than within the sheets (the weaker attractions don't
hold atoms as close). Second, the sheets are able to slip past each other easily because
the attractions are weak all along the layers. For this reason, the imaginary planes that
run through the graphite sheets are called "glide planes." Glide planes are present
anytime the attractions along one plane are weaker than any other planes in the
substance. The extensive glide planes in graphite are responsible for the softness and
lubricating qualities of graphite.
Experimental Procedures:
Harvesting seed crystals
Inspect the second and third beakers for the best seed crystal of potassium
ferricyanide and alum, respectively. Good seed crystals should be approximately 3
mm long and not be stuck to other crystals. Also, make sure there are no
discontinuities or breaks within the crystal as this may be an indication of more than
one crystal being present (hold the crystal up to the light to assist you in this process).
The crystal does not need to be well shaped at this point.
After applying a small amount of Duco-cement to a thread (enough to cover the entire
tip of the thread), touch the end firmly to the seed crystal. Allow the cement to harden
between the crystal and the thread. In the meantime you may make up your crystal
growing solutions and build some model structures (see further below).
Because we consume a great deal of chemicals while making our crystals, we will
attempt to reduce our chemical consumption by reusing as much of our solutions as
possible. If there is any solution left in the second and third beakers, transfer these
solutions to similarly marked 400 mL beakers. You will need solutions with a final
total volume of 150 mL each, so for each additional mL of water added to each
solution, you must add 0.5g K3Fe(CN)6 or 0.18g KAl(SO4)2.12H2O. You may use
the solid that has already precipitated at the bottom of the earlier beakers as part of the
solid added.
As before, stir and heat your solutions until the solids completely dissolve, then set
aside to cool. (Warning: It is very important that the solutions are completely cooled
before adding the seed crystals. If they are not, the crystals will redissolve). Proceed
to the model building portion of this lab.
When the solutions have been completely cooled, bend a piece of copper wire around
the lip of the beakers so the watch glasses can still fit on top. It is all right if there is a
small space between the beaker and watch glass due to the wire. Tie the opposite end
of each seed crystal thread around one of the copper wires and adjust the length of the
thread such that the seed crystal will be suspended as close to the center of the
solution as possible (Figure 4). You may want to cut the excess thread to avoid
dangling it in the solution and having it become an unwanted crystallization site.
Again, cover each beaker with a watch glass and let them sit undisturbed in your lab
drawer over the next week. Refer to the diagram below to make sure you have the
correct setup. The NaNO3 beaker should have crystals starting to grow already, and
these should also be left until the next session.
Leave your graphite and MoS2 models constructed so you can refer to them in the
next section.
Model Building - Molecular Modeling Kit
Due to limited time and resources, half of the class will build graphite, and the other
half will build diamond. Match up with another group of students so you can pool the
resources from two model kits. The black spheres in your kits represent carbon atoms,
and you will be using them exclusively. The shorter connectors represent single bonds
, while two of the longer connectors are used for double bonds. You will need to use
parts from more than one kit to build your models, so, please make sure that all of the
pieces are returned to your kit at the end of the lab. Each kit should contain 14 black
carbon atoms, roughly 40 single bonds, and 12 double bonds.
Graphite
Start by building a ring of carbons in which every other bond is a double bond. Note
that your ring of carbons all lie in the same plane. The students who are working on
diamond are also building rings of six carbons, but, their carbon atoms lie in different
planes. Continue building rings off of each other until you have a structure containing
seven fused rings like one of the figures below. Dotted lines have been added to show
that the actual structure of graphite continues far beyond the section you are building.
The third structure in Figure 4 is blank, and you may use it to construct a blueprint for
your structure if you wish.
frequently in chemistry, and oftentimes chemists notate average bonds in graphite and
similar structures by placing a circle inside each ring of carbon:
Figure 8. The two possible overhead views of the base for a larger diamond model.
The o's represent locations where bonds will extend upwards.
Make sure that all three rings are in the same plane. If one of the rings points
downwards, you haven't connected them correctly. As a group, build the next layer up
to complete three structures like the one in Figure 7. Complete the "pyramid" by
adding a top layer. Your structure should be large enough that you can continue the
repeating pattern on your own. Extend your model by as many carbon atoms as you
have left in your kits. Have your lab instructor check your structure when you are
done.
Glide Planes in MoS2 (both groups)
Compare the structure of graphite (if you didn't build it, find a group that did) to that
of MoS2. Locate the glide plane in MoS2. Remember that the solid state kits do not
show bonds between atoms, so you may want to consult with your lab instructor
before making up your mind. Draw a diagram of the glide plane in MoS2 in your
notebook.
Questions
1) Both the graphite structure and the diamond structure contain rings of six carbon
atoms. In graphite, the carbon atoms in each ring all lie in the same plane, while in
diamond, the carbon atoms are in different planes (they are staggered). Explain why
these rings have different shapes.
2) The distance between two bonded carbon atoms in graphite is about 1.4x10 -10
meters. The distance between the carbons in your graphite model is approximately
0.04 m. So, the scaling factor for the model is roughly 3x108 larger than graphite on
the true atomic level. Find the diameter of the model necessary to represent a pencilpoint of graphite, if the dot is 1mm in diameter (0.01m) If there are about 1600 meters
in a mile, convert your value to miles. Describe a distance that you are familiar with
that is comparable to this amount.
3) Diamonds are routinely cut into various shapes to form jewelry pieces. Do you
think the cutting process is an example of gliding or cleaving? Defend your choice.
4) Diamonds have the unusual property that they fluoresce (give off light) when
subjected to x-rays. This property is exploited in the diamond mining process to detect
diamond deposits. Unfortunately, zirconium is another substance which fluoresces in
the same way under x-rays, and is often found in diamond mines as well. Speculate on
some ways that the zirconium and diamond could be separated after being detected by
the x-ray process. You can just brainstorm, you don't need to look up anything about
zirconium.
5) Considering diamond and graphite, which structure seems to be more dense?
Suppose you are given samples of graphite and diamond. Describe a method that you
could use to determine their densities from these samples. Describe another method
you could use to determine their densities just from the models you have built. Have
your lab instructor give you feedback on your ideas.
SESSION #3
Objectives
* Gather the large single crystals and compare their shapes
* Build models to demonstrate cleavage planes
* Study the properties of some substances studied in the lab
Crystal Shapes
Of the crystals you have grown, NaNO3 has the simplest shape on the atomic level. It
is similar to the NaCl structure in that the chloride (Cl-) ions of NaCl are "replaced"
by nitrate (NO3-) ions. Nitrate is an example of a polyatomic ion, which means that
the ion unit is composed of several atoms, not just one atom like chloride (Cl-). Nitrate
ions have a triangular shape which causes the repeating units in NaNO3 to distort
from a cube-like shape to a rhombohedron. The diagrams below show the repeating
units for NaCl and NaNO3 for comparison. Overhead views of the top and second
layer of the repeating pattern are shown as a visual aid (note that the bottom layer is
the same as the top layer). The shape of the repeating pattern is also given at the far
right. The macroscopic shapes of the crystals you have grown are related to the
repeating pattern of atoms, and also on the growth rate of each of the crystal faces.
In this diagram, you can think of the large spheres as being chloride ions and the
smaller spheres as the sodium ions. So, what happens when you apply a cleaving
force? STEP 1 in the diagram is immediately before the cleaving force has been
applied. STEP 2 shows atoms shifting downward as a result of the applied force. Note
that this position puts the same charges opposite each other. Similar charges repel
each other, leading to STEP 3 where the solid breaks along the cleaving plane. You
should note that for the diagram above, there is also a cleaving plane horizontally
through the substance. What happens if the applied force is not exactly along the
cleaving plane? As you might expect, forces not directly along cleaving planes are not
as effective. But, if cleaving does occur it will always occur down cleavage planes.
Some solids can contain both cleavage planes and glide planes. Both types of planes
are convenient places for the substance to break. The important difference between
the two types is what occurs on the microscopic level. Glide planes result due to weak
attractions along a plane, while cleavage planes occur when strong repulsions result
through motion along the plane.
Materials Testing
You will test the hardness of graphite and diamond which you have been investigating
in lab. A convenient (though informal) scale for measuring the hardness of materials is
Moh's hardness scale. Some common materials and their Moh hardness value are
listed below.
Table 2. Moh's Hardness Scale
Material
Hardness
Alum
2 - 2.5
Copper
2.5 - 3
Diamond
10
Graphite
0.5 - 1
Iron
4-5
Lead
1.5
Quartz
Rock salt
Wax
0.2
Higher numbers correspond to harder substances. When two different substances are
rubbed together, the substance with the lower hardness value will be scratched by the
other. Diamond is currently accepted as the hardest known material.
Experimental Procedures:
kind has an "x" shape. Your lab partner concludes that the substance grows two
fundamentally different shapes of crystals. What do you think? Give an alternate
explanation for the two shapes.
3) Your lab partner has somehow broken a piece of seaborgium chloride, but, doesn't
have any recollection of the process. Your lab partner believes that since the two
pieces of seaborgium chloride look identical that the breaking process must have been
due to gliding. Explain if this is necessarily true. What should you do to prove or
disprove your lab partner.
Reference (1) Values obtained from the CRC Handbook of Chemistry and Physics,
65th Edition, Robert C. Weast, Melvin J. Astle, and William H. Beyer (editors), CRC
Press Inc., Boca Raton, 1984.